反应详情

(3aRS,7aRS)-2-Benzyl-7,7-diphenylperhydro-4-isoindolone (150 g), methanol (1500 cc) and 1N hydrochloric acid (450 cc) are added to palladinized charcoal (10% palladium) (15 g); the reaction mixture is hydrogenated with stirring at room temperature and at atmospheric pressure. After 5 hours' reaction, the theoretical volume of hydrogen has been absorbed; the reaction mixture is filtered, then concentrated to dryness under reduced pressure (2.7 kPa); the residue is crystallized in ethanol (200 cc). The crystals obtained are drained, washed with ethanol (50 cc) and dried. (3aRS,7aRS)-7,7-Diphenylperhydro-4-isoindolone hydrochloride (110 g), m.p. 270° C. with decomposition, is obtained.

1. customAfter 5 hours' reaction
2. customthe theoretical volume of hydrogen has been absorbed
3. filtrationthe reaction mixture is filtered
4. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
5. customthe residue is crystallized in ethanol (200 cc)
6. customThe crystals obtained
7. washwashed with ethanol (50 cc)
8. customdried